CN115367773A - Environment-friendly L-carnitine production process - Google Patents
Environment-friendly L-carnitine production process Download PDFInfo
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- CN115367773A CN115367773A CN202211039443.2A CN202211039443A CN115367773A CN 115367773 A CN115367773 A CN 115367773A CN 202211039443 A CN202211039443 A CN 202211039443A CN 115367773 A CN115367773 A CN 115367773A
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- ammonium chloride
- sodium chloride
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- carnitine
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/26—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing carboxyl groups by reaction with HCN, or a salt thereof, and amines, or from aminonitriles
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Abstract
The invention belongs to the technical field of food additives and pharmaceutical chemicals, and particularly relates to a green and environment-friendly L-carnitine production process. The green and environment friendly L-carnitine producing process includes the reaction of ammonium chloride produced through hydrolysis of L-carnitine and certain amount of sodium nitrite at 50-70 deg.c for 1-3 hr to convert into non-toxic and harmless directly dischargeable nitrogen gas and obtain sodium chloride. According to the invention, a large amount of ammonium chloride generated by hydrolysis of nitrile in the L-Cara is subjected to harmless green environmental protection treatment, the mixed salt of sodium chloride and ammonium chloride is changed into a pure resource product, namely sodium chloride, which can be directly utilized, and meanwhile, the discharged nitrogen is nontoxic and harmless, so that the ammonia nitrogen problem is solved ingeniously, and finally, the ammonia nitrogen concentration of the sewage reaches below 15mg/L of the primary discharge standard of the integrated wastewater discharge standard GB 8978-1996, and the method has important practical value and economic value.
Description
Technical Field
The invention belongs to the technical field of food additives and pharmaceutical chemicals, and particularly relates to a green and environment-friendly L-carnitine production process.
Background
In the production process of L-carnitine, most manufacturers adopt the following production processes: a. amination (S-epoxy and trimethylamine hydrochloride are synthesized into L-quaternary ammonium salt), b, cyaniding (L-quaternary ammonium salt and sodium cyanide are synthesized into L-Carnean nitrile), c, hydrolysis addition (L-Carnean nitrile is hydrolyzed into L-carnitine hydrochloride), d, desalting (most of sodium chloride and a small amount of ammonium chloride mixed salt are removed) e, ion exchange (the L-carnitine is obtained), f, and wastewater treatment (sodium chloride and ammonium chloride mixed salt are recovered from concentrated salt-containing wastewater). A large amount of energy is consumed when the salt-containing wastewater is concentrated, and meanwhile, the cost is increased; the obtained mixed salt of sodium chloride and ammonium chloride can not be directly used as a resource, and can be used only by further separation and purification, which increases a great deal of cost.
Therefore, a green and environment-friendly L-carnitine production process is urgently needed to change the mixed salt of sodium chloride and ammonium chloride into a pure resource product which can be directly utilized.
Disclosure of Invention
The invention aims to provide a green and environment-friendly L-carnitine production process, which is used for performing harmless green and environment-friendly treatment on a large amount of ammonium chloride generated by hydrolysis of L-Carnitine in the L-Carnitine production process.
The technical scheme provided by the invention is that the L-carnitine production process is environment-friendly, ammonium chloride generated after hydrolysis of L-Carnitril reacts with a certain amount of sodium nitrite at 50-70 ℃ for 1-3 hours, and the ammonium chloride is converted into non-toxic harmless nitrogen which can be directly discharged, and sodium chloride is obtained.
Further, the amount of sodium nitrite is such that 99% of the ammonium chloride equivalent is converted to sodium chloride and nitrogen.
Further, the reaction temperature is preferably 55 to 60 ℃.
Further, the reaction time is preferably 2 hours.
The sodium pyrosulfite is used for removing crotonobetaine impurities generated in hydrolysis, and a small part of L-carnitine is hydrolyzed for a long time and at a high temperature to remove one molecule of water to become impurity crotonobetaine.
Methanol is a solvent in desalting, most of water is concentrated and distilled away, and then methanol is added, so that the solubility of sodium chloride and ammonium chloride in methanol is low, and the solubility of L-carnitine is high, so that most of salt can be removed.
Desalting is to evaporate most of the water, crystallize sodium chloride and ammonium chloride, and then separate L-carnitine from methanol.
Compared with the prior art, the invention has the beneficial effects that.
According to the invention, a large amount of ammonium chloride generated by hydrolysis of nitrile in the L-Cara is subjected to harmless green environmental protection treatment, the mixed salt of sodium chloride and ammonium chloride is changed into a pure resource product, namely sodium chloride, which can be directly utilized, and meanwhile, the discharged nitrogen is nontoxic and harmless, so that the problem of ammonia nitrogen is solved skillfully, the ammonia nitrogen concentration of the sewage finally reaches below 15mg/L of the primary discharge standard of the integrated sewage discharge standard GB 8978-1996, and the method has important practical value and economic value.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a flow chart of the process of the prior art.
Detailed Description
The invention is further illustrated by the following examples. It is to be understood that the embodiments described are only some embodiments of the invention, and not all embodiments.
Example 1.
Hydrolysis of one ton of L-endocarbonitrile yields 299.7Kg of ammonium chloride, which after hydrolysis is adjusted to pH 6.5 with sodium hydroxide solution, which yields about 328.0Kg of sodium chloride, both of which yield 627.7Kg of mixed ammonium chloride and sodium chloride salts. Then carrying out the next addition reaction, after the addition reaction is finished, adding 382.7Kg of sodium nitrite, heating to 60 ℃ in a reaction tank for 2 hours to react, so that 99.0 percent of ammonium chloride is converted into 324.4Kg of sodium chloride and 155.3Kg of nitrogen, the nitrogen is harmless and is directly discharged into the air, and 610Kg of pure sodium chloride is separated during desalting. And finally, about 3.0Kg of ammonium chloride and 42.4Kg of sodium chloride are discharged from the sewage, the corresponding amount of discharged sewage is 100 tons, and the ammonia nitrogen generated by the ammonium chloride is 9.5mg/L and is less than 15mg/L of the primary discharge standard of GB 8978-1996. Because insufficient sodium nitrite is used for reaction with ammonium chloride, the sodium nitrite is completely consumed, and detection and assay show that no sodium nitrite is present in the sewage, so that no hidden danger exists in the biochemical treatment of the sewage in the later period.
Example 2.
Hydrolysis of one ton of L-endocarbonitrile yields 299.7Kg of ammonium chloride, which after hydrolysis is adjusted to pH 6.5 with sodium hydroxide solution, which yields about 328.0Kg of sodium chloride, both of which yield 627.7Kg of mixed ammonium chloride and sodium chloride salts. Then carrying out the next addition reaction, after the addition reaction is finished, adding 382.7Kg of sodium nitrite, heating to 55 ℃ in a reaction tank for reaction for 3 hours to convert 99.0 percent of ammonium chloride into 324.4Kg of sodium chloride and 155.3Kg of nitrogen, directly discharging the nitrogen which is a harmless substance into the air, and separating 610Kg of pure sodium chloride during desalting. And finally, about 3.0Kg of ammonium chloride and 42.4Kg of sodium chloride are discharged from the sewage, the corresponding discharged sewage amount is 100 tons, and the ammonia nitrogen generated by the ammonium chloride is 9.5mg/L which is less than the primary discharge standard of GB 8978-1996 of 15mg/L. Because insufficient sodium nitrite is used for reaction with ammonium chloride, the sodium nitrite is completely consumed, and detection and assay show that no sodium nitrite is present in the sewage, so that no hidden danger exists in the biochemical treatment of the sewage in the later period.
Example 3.
Hydrolysis of one ton of L-endocarbonitrile yields 299.7Kg of ammonium chloride, which after hydrolysis is adjusted to pH 7.0 with sodium hydroxide solution, which yields about 328.0Kg of sodium chloride, both of which yield 627.7Kg of mixed ammonium chloride and sodium chloride salts. Then carrying out the next addition reaction, after the addition reaction is finished, adding 382.7Kg of sodium nitrite, heating to 60 ℃ in a reaction tank for 2 hours to react, so that 99.0 percent of ammonium chloride is converted into 324.4Kg of sodium chloride and 155.3Kg of nitrogen, the nitrogen is harmless and is directly discharged into the air, and 610Kg of pure sodium chloride is separated during desalting. And finally, about 3.0Kg of ammonium chloride and 42.4Kg of sodium chloride are discharged from the sewage, the corresponding discharged sewage amount is 100 tons, and the ammonia nitrogen generated by the ammonium chloride is 9.5mg/L which is less than the primary discharge standard of GB 8978-1996 of 15mg/L. Because insufficient sodium nitrite is used for reaction with ammonium chloride, the sodium nitrite is completely consumed, and detection and test show that no sodium nitrite exists in the sewage, and no hidden trouble exists in the biochemical treatment of the sewage in the later period.
Example 4.
Hydrolysis of one ton of L-endocarbonitrile yields 299.7Kg of ammonium chloride, which after hydrolysis is adjusted to pH 7.0 with sodium hydroxide solution, which yields about 328.0Kg of sodium chloride, both of which yield 627.7Kg of mixed ammonium chloride and sodium chloride salts. Then, the next addition reaction is carried out, after the addition reaction is finished, 382.7Kg of sodium nitrite is added, the mixture is heated to 45 ℃ in a reaction tank for reaction for 3 hours, 97.0 percent of ammonium chloride is converted into 317.9Kg of sodium chloride and 152.2Kg of nitrogen, the nitrogen is harmless and is directly discharged into the air, and 608Kg of pure sodium chloride is separated during the desalting. And finally, 9.0Kg of ammonium chloride, 40.4Kg of sodium chloride and 7.8 Kg of sodium nitrite are discharged from the sewage, the corresponding discharged sewage amount is 100 tons, and the ammonia nitrogen generated by the ammonium chloride is 28.6mg/L which is more than 15mg/L of the primary discharge standard of GB 8978-1996. Because unreacted sodium nitrite is remained at 7.8 Kg, the sewage can not be directly discharged, otherwise, the potential hazard exists in the biochemical treatment of the sewage in the later period, and the sodium nitrite can inhibit or kill the biological flora in the sewage biochemical pool.
Example 5.
Hydrolysis of one ton of L-endocarbonitrile yields 299.7Kg of ammonium chloride, which after hydrolysis is adjusted to pH 7.0 with sodium hydroxide solution, which yields about 328.0Kg of sodium chloride, both of which yield 627.7Kg of mixed ammonium chloride and sodium chloride salts. Then carrying out the next addition reaction, after the addition reaction is finished, adding 382.7Kg of sodium nitrite, heating to 75 ℃ in a reaction tank for 2 hours to react so as to convert 99.0 percent of ammonium chloride into 324.4Kg of sodium chloride and 155.3Kg of nitrogen, directly discharging the nitrogen which is a harmless substance into the air, and separating 610Kg of pure sodium chloride during desalting. And finally, about 3.0Kg of ammonium chloride and 42.4Kg of sodium chloride are discharged from the sewage, the corresponding discharged sewage amount is 100 tons, and the ammonia nitrogen generated by the ammonium chloride is 9.5mg/L which is less than the primary discharge standard of GB 8978-1996 of 15mg/L. Because insufficient sodium nitrite is used for reaction with ammonium chloride, the sodium nitrite is completely consumed, and detection and assay show that no sodium nitrite is present in the sewage, so that no hidden danger exists in the biochemical treatment of the sewage in the later period. However, in the presence of sodium nitrite, the temperature is too high (higher than 70 ℃), which increases a small amount of impurity-crotonobetaine in the L-carnitine, and is not favorable for the quality of the L-carnitine product.
Example 6.
Hydrolyzing one ton of L-Carlactonitrile according to the existing manufacturer's production process to generate 299.7Kg of ammonium chloride, after the hydrolysis is finished, adjusting the pH value to 7.0 with sodium hydroxide solution, and generating about 328.0Kg of sodium chloride, and forming 627.7Kg of mixed salt of ammonium chloride and sodium chloride. And then carrying out the next addition reaction, and desalting after the addition reaction is finished to separate 510Kg of mixed salt of ammonium chloride and sodium chloride. And finally, about 84.7Kg of ammonium chloride and 33.0Kg of sodium chloride are contained in the wastewater, if the wastewater is directly discharged at the moment, the corresponding discharged sewage amount is 100 tons, the ammonia nitrogen generated by the ammonium chloride is 269.0mg/L which is far higher than the 15mg/L of the primary discharge standard of GB 8978-1996, and the wastewater cannot be directly discharged. Therefore, concentration and desalination equipment is required to be added, investment is increased, energy consumption is greatly improved, labor cost is increased, and profits of enterprises are reduced. The obtained ammonium chloride and sodium chloride mixed salt product can not be directly used, and needs to be further processed to separate pure sodium chloride and ammonium chloride, and needs to invest equipment, plants and production posts, and simultaneously increases the production cost and reduces the profit of enterprises again.
The above-described examples are intended to be illustrative of one embodiment of the present invention and are not intended to be limiting thereof. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (4)
1. A green and environment-friendly L-carnitine production process is characterized in that ammonium chloride generated after hydrolysis of nitrile in L-Cara reacts with a certain amount of sodium nitrite at 50-70 ℃ for 1-3 hours to be converted into nontoxic and harmless nitrogen which can be directly discharged, and sodium chloride is obtained.
2. The process of claim 1, wherein the amount of sodium nitrite is such that 99% of the ammonium chloride equivalent is converted to sodium chloride and nitrogen.
3. The process of claim 1, wherein the reaction temperature is preferably 55-60 ℃.
4. The process of claim 1, wherein the reaction time is preferably 2 hours.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583816A (en) * | 2012-01-30 | 2012-07-18 | 西安石油大学 | Method for reusing and treating oily wastewater by adopting nitrogen gas floatation technology |
| CN113698320A (en) * | 2021-09-23 | 2021-11-26 | 抚顺顺能化工有限公司 | Preparation method of L-Carlactonitrile |
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- 2022-08-29 CN CN202211039443.2A patent/CN115367773A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583816A (en) * | 2012-01-30 | 2012-07-18 | 西安石油大学 | Method for reusing and treating oily wastewater by adopting nitrogen gas floatation technology |
| CN113698320A (en) * | 2021-09-23 | 2021-11-26 | 抚顺顺能化工有限公司 | Preparation method of L-Carlactonitrile |
Non-Patent Citations (1)
| Title |
|---|
| 王业飞等: "亚硝酸钠与氯化铵体系的反应特征", 《石油学报》, pages 226 - 234 * |
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